Methyl iodide → HCID 12395564, 화합물

HRID 597006노트

반응식

HRID 597006 반응식
[CH:1]([CH:4]1[CH2:12][C:11]2[C:6](=[C:7]([Cl:16])[C:8]([Cl:15])=[C:9]([O:13][CH3:14])[CH:10]=2)[C:5]1=[O:17])([CH3:3])[CH3:2].[H-].[Na+].[CH3:20]I>COCCOC>[CH3:20][C:4]1([CH:1]([CH3:3])[CH3:2])[CH2:12][C:11]2[C:6](=[C:7]([Cl:16])[C:8]([Cl:15])=[C:9]([O:13][CH3:14])[CH:10]=2)[C:5]1=[O:17]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 12395556HCID 12395556, 화합물

생성물 1

HCID 12395564HCID 12395564, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
30 °C

실험 절차

A stirred suspension of 2-isopropyl-5-methoxy-6,7-dichloro-1-indanone (7.3 g., 0.025 mole) and sodium hydride (810 mg., 0.028 mole) in anhydrous 1,2-dimethoxyethane(250 ml.) is heated in an inert atmosphere at 80°-85° C. for 1 hour, cooled to 30° C. and treated with methyl iodide (6 ml.). The reaction mixture is heated to 80° C., then the solvent is distilled at reduced pressure and the residue poured into ice water. The 2-methyl-2-isopropyl-5-methoxy-6,7-dichloro-1-indanone which separates (7.0 g.) melts at 143° C. after recrystallization from ethanol-water.

후처리

  1. temperatureis heated in an inert atmosphere at 80°-85° C. for 1 hour
  2. temperatureThe reaction mixture is heated to 80° C.
  3. distillationthe solvent is distilled at reduced pressure
  4. additionthe residue poured into ice water
  5. customafter recrystallization from ethanol-water

출처 및 근거

ORD 기록
ord-1011dfa3b05c45b89c38cfa8784bc84a
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012524

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